HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 67454300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethoxalyl chloride | HCID 20884 | — |
| Reactant | 2,4-Difluorobenzamidoxime | HCID 2823825 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67454300 | HCID 67454300 | 77.3% |
Reaction Steps
To a solution of 2,4-difluoro-N′-hydroxybenzimidamide 5.2 (3.52 g, 33% purity, max. 7.2 mmol) and pyridine (2.32 mL, 28.7 mmol) in anhydrous CH2Cl2 under N2 was added ethyl chlorooxoacetate (1.27 g, 9.32 mmol) dropwise over 5 min at RT. The mixture was stirred under reflux. After 1 h30, the rxn mixt. was concentrated and purified on silica gel using CH2Cl2, furnishing 1.414 g of title product 5a as colorless oil. Yield: 1.414 g (78%). LCMS: P=94%, rt=4.21 nm, m/z=255, 277 (M+Na).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871761B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-646eaa8e66ef488aa7137e19c8d57fa6 |
| Source note | uspto-grants-2014_10 |